Manufacture of black coloring-matters.



WTTEE E MANUFACTURE 0 BLACK COLORING-MiXTTERS.

arissa.

15o Drawing.

To all whom it may concern:

Be itknown that we, Josurn TURNER and HARRY DEAN, subjects of KingGeorge V of Great- Britain, residing at Huddersfield, in the county ofYork, England, have invented certain new and useful Improvements in theManufacture of Black Coloring-Matters, of which the following is aspecification.

Our invention relates to the production of black coloring matters fordyeing cotton pr vegetable fibers directly deep black shades.

In our experiments, we have found that chlor-metwphenylenediamin is verysuitable for use as an end component in the manufacture of blackdyestuffs which dye gptton or vegetable fibers directly and posess greatatlinity therefor. For instance, we take a para-mono-amido-azo compoundsuch as para amido benzene azo alpha nap-hthylamin-sulfonic-acidprepared say by the action of diazotized para-amido-acetani' lid uponalpha-maphthylamin-sulfonic-acid- 1-6 or 1-7 (Cleves acids) andsubsequent hydrolysis. The said para-amido-azo compound is treated withone molecule or" nitrous acid, preferably not above 5 C., at whichtemperature the amide group of the benzene nucleus only is attacked. The

formed diazo compound is then combinedwith one molecule ofamido-naphthol-monosulfo acid (28.6) (G acid) in alkaline solution. Whenthe combination is complete the intermediate dyest-ull is furtherdiazot-ized with one molecule of nitrous acid and combined with onemolecule of chlor-metaphenylene-diamin. The chlor-meta-phenylene-diaminis prepared by reducing in the ordinary way dinitro-chlor benzol.

To enable ourinvention to be fully understood, we will give an exampleof the manufacture of black coloring matters in accordance therewith.7.28 kilos of sodium salt ofpara-amido-benzene-azo-alpha-naphthylamin-sulfo-acid 1-6 or 1-7 aredissolved and the solution carefully precipitated with 5.2 kilos H01 atatemperature between 0 and Specification of Letters Eatent. Applicationfiled April 24, 1911. Serial in). ocean.

"Patented. J an. 15%,

o C. At this temperature there is run in slowly a solution of 1.4 kilosnitrite of soda. The agitator is then allowed to run until a test showsonly a trace of free nitrous acid. The thus produced amido-diazocompound is run into a cold solution of 5 kilos-amidonaphthol-sulfo-acid(2.8.6.) (G acid) the solution being kept alkaline by means of sodiumcarbonate or ammonia. As soon as the combination is completed the violetblack intermediate compound is further diazotized by means of 1.4 kilosnitrite of soda and 5.2 kilos 1101.

When the mixture shows no trace of nitrous acid, it is run into analkaline solution containing 2.86 chlormeta-phenylene-diamin 1:2 :4. Thecoloring matter may be separated by the addition of salt, and byfiltering, pressing, and drying.

Having thus described our invention, what I we claim as new and desireto secure by Letters Patent is 1. A process for manufacturing adyestufi' which consists in combining a diazo compound with one moleculeof amido naphthol mono sulfonic acid (2.8.6) (G acid), furtherdiazotizing the intermediate body thus formed, and finally combining itwith one molecule of chlor meta phenylene diamin 1 :2 :4 in alkalinesolution.

which consists in first treating a para amido azo compound with onemolecule of nitrous acid, then combining the diazo compound thus formedwith one molecule of amido naphthol mono sult'onic acid (2.8.6) (Gacid), further diazot-izing the intermediate body thus formed, andfinally combining it with one molecule of chlor meta phenylene diamin1:2 :4 in alkaline solution.

In testimony whereof we aflix our signatures in the presence of twowitnesses.

JOSEPH TURNER. HARRY DEAN. lVitnesses:

Fnnnnmcn I. BRIGHT, THOMAS H. BARRON.

a. A process for manufacturing a dyestulf

